CN102995066A - Molten salt electrochemical reduction method for removing sulfide inclusions on solid steel surface - Google Patents
Molten salt electrochemical reduction method for removing sulfide inclusions on solid steel surface Download PDFInfo
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Abstract
The invention relates to a method for removing sulfide inclusions on solid steel surface by molten salt electrochemical reduction process, belonging to the field of clean steel. In the method, chloride is used as a molten salt electrolyte, the electrolysis temperature of molten salt is 800-900 DEG C, the electrolysis voltage is 2.0-4.0V, and the electrolysis time is 1-3 hours. Specifically, the chloride of alkali metal and alkaline earth metal is used as the molten salt system, the cathode is the solid steel containing sulfide inclusions, and the anode is high-purity graphite. In the electrolysis process, inert gas is used for protection; water cooling is carried out; and quartz, glass or stainless steel is used as the raw material for the inner shell of an electrolytic bath. When carrying out pre-electrolysis, a graphite carbon rod is used as the anode, and a Fe-Cr-Al wire is used as the cathode. After pre-electrolysis, the graphite anode and the prepared cathode steel sample are inserted into the molten salt for executing electrolysis through the direct current, and in the whole process, high-purity argon is always needed to be introduced into the reactor. The sulphur content of the steel sample after electrolysis is reduced greatly, so that the steel sample can meet the requirements on special application of steel. The method shows that the molten salt electrochemical reduction method has the effect of remarkably removing the sulfide inclusions on the solid steel surface. The method can provide a new way of removing sulfide inclusions on the solid steel surface for the domestic iron and steel field, and has great practical significance in saving energy, reducing emission, improving efficiency, reducing pollution, and the like.
Description
Technical field
The invention belongs to the Clean Steel field, be specifically related to utilize the molten salt electrochemistry reduction process to remove the method for the sulfide inclusion on solid steel surface.
Background technology
Along with developing rapidly of modern industry production and science and technology, the requirement of steel product quality is improved day by day.Produce internal fissure and obtain good surface quality for fear of steel billet, require the sulphur content of ordinary steel less than 0.020%; In order to make structure iron have uniform mechanical property, require in the steel sulphur content less than 0.010%; In order to make oil and natural gas transfer lime, petroleum refining unit have the impelling strength of anti-Hydrogen induced cracking performance, more uniform mechanical property and Geng Gao with steel etc. with steel, Cryogenic Steel, medium-thickness ship plate steel and aviation with steel, offshore production platform, silicon steel has good electromagnetic performance, sheet steel has good deep drawability etc., requires in the steel sulphur content less than 0.005%.For this reason, in the production of steel, develop hot metal pretreatment before the steel-making and the liquid steel refining technology after the steel-making removing unnecessary sulphur, satisfied the Finished Steel specification requirement.
But, for some effects on surface performance steel and the parts of particular requirement are arranged, take expensive deep desulfuration obviously uneconomical.Sulfide inclusion seriously influences the antiseptic property of steel, even the sulphur of low levels also can cause the corrosion failure of steel surface or produce defective.This is because there is the difference of current potential between the inclusion of steel surface and matrix, surface-area different and lack protective membrane, and the sulfide ratio that these are mingled with is easier to be dissolved in the water.In case the dissolving of inclusion occurs, the metallic surface just produces a large amount of corrosion pits, thereby has accelerated its further corrosion, has a strong impact on its intensity and surface property, and its range of application is restricted, and more is difficult to normal military service when using under some particular surroundingss.Requiring with steel of some special dimensions is more harsh, such as automobile and instrument steel plate.Although people have adopted the content of a lot of methods minimizing inclusiones, because the Iron and Steel Production scale is large, process is complicated, can not contained the steel of any inclusion.Therefore how to reduce in steelmaking process the sulfide inclusion generation except research, how research removes the sulfide inclusion of some solid-state surface of steel plate in order to improve anticorrosion and other performance of material, and it also is very necessary satisfying special needs.The electrochemical reduction technology may be a kind of desirable method.
Electrochemistry is widely used in field of metallurgy.Its application mainly is divided into two aspects, and the one, electrolytic reduction prepares metal, such as the production of aluminium; The 2nd, for the electrochemistry refining.In the electrochemistry refining process, will treat that normally the metal of refining is made anode, pure metal carries out electrolysis as negative electrode.The at first oxidation of the metal of anode enters solution with the form of ion, and then these ions are in cathodic reduction.In the aqueous solution refined matte and in fused salt refined aluminum be exactly this situation.Yet, if in refining process, a small amount of impurity is directly removed from metal, upward still from cost, all very large advantage can be arranged and stay pure metal from energy-conservation.According to this idea, the someone begins the research of this respect in molten salt system.
The G.Chen of Cambridge University and D J Fray have developed Direct Electrolysis reduction TiO in molten chloride accordingly
2Produce the technique of metal titanium, be called as " FFC Cambridge technique ".In this technique, titanium dioxide is made into electrolysis cathode, and graphite is made anode, and electrolytic solution is the CaCl of melting
2, after an amount of electric current passed through, oxonium ion left oxide compound, was diffused into the anode place, was combined into CO with carbon and overflowed, and metal titanium is then stayed negative electrode.Not have liquid titanium or ion titanium in this process with the key distinction of traditional electrolysis process.Although TiO
2Specific conductivity is lower, but still can be used as effective negative electrode.In case this is because oxygen is emitted, there is metal titanium to generate, its electroconductibility improves greatly, and reaction can be carried out smoothly.This technique is a kind of method of low-cost electrochemical production titanium.The advantage of this technology is:
(1) greatly reduces raw materials cost, take titanium as criterion calculation, approximately reduce by 50%;
(2) greatly reduce oxygen level in the titanium, technique in the past can't resolve the high problem of oxygen level;
(3) explained hereafter cycle weak point, product is applicable to powder metallurgy formation;
(4) this technique also is applicable to the preparation of other metal that multiple preparation is difficult, cost is high, activity is strong.
Therefore, the method also should be removed the sulphur in the solid matter in fused salt.
The present invention removes the inclusion on solid steel surface by the molten salt electrochemistry reduction technique, and the sulfur-bearing inclusion that overcomes the steel surface is existing corrosion and strength problem in use.Not only can improve the antiseptic property of material surface, and overcome other defective of material, will greatly be prolonged the work-ing life of material.The invention achievement has the superiority such as technique is simple, cost is lower, and for developing new technology, the application of novel process in steel industry, energy-saving consumption-reducing is raised the efficiency, and minimizing pollution etc. all has great practical significance.For being mingled with, removal solid steel surface sulfide thing provides a new way and reliable scientific basis.What the gained steel especially can satisfy many special dimensions uses the steel requirement, such as automobile and instrument steel plate.Therefore have broad application prospects and scientific meaning.
Summary of the invention
The object of the invention is to large in the Iron and Steel Production scale, process is complicated, can not do not contained on the prerequisite basis of steel of any inclusion, avoided taking the traditional way of expensive deep desulfuration, a kind of technique is simple, cost is mingled with than lowland removal solid steel surface sulfide thing new way, novel method are provided.
Technical scheme of the present invention and technical characterictic are:
The present invention utilizes the molten salt electrochemistry reduction process to remove the method for the sulfide inclusion on solid steel surface, it is characterized in that selecting muriate as molten salt electrolyte, the temperature of fused salt electrolysis is 800 ℃～900 ℃, and electrolysis voltage is 2.0～4.0V, and electrolysis time is 1 hour～3 hours.The method of the sulfide inclusion on this removal solid steel surface may further comprise the steps: fused salt is chosen and pre-treatment; Preelectrolysis and electrolytic process.
Used fused salt is the muriate of alkali and alkaline earth metal ions, selection principle is: have the characteristic of non-toxic inexpensive, more stable chemical property, higher vapour pressure, less viscosity, higher conductance, with large by the density difference of Electrowinning metal, more greatly, easily electrolysate is in time separated to the interfacial tension of metal, the ability that has simultaneously stronger dissolved substance is beneficial to electrolytic process and carries out.
Used negative electrode is that sulfur-bearing is mingled with solid steel, and used anode is high purity graphite.In the electrolytic process react into:
Cathodic reaction:
FeS+2e→Fe+S
2- (1)
S+2e→S
2- (2)
Anodic reaction:
(S
2-)
Sulfide→ (S
2-)
In the fused salt(3)
CaCl
2-2e →Ca
2++Cl
2↑ (4)
Total reaction:
CaCl
2+FeS→CaS+Fe+Cl
2↑ (5)
The step of the thionic in the steel sample is removed in reaction (1) and reaction (2).Reaction (3) is diffused in the fused salt sulfonium ion in the cathode steel sample.Reaction (4) is that the ion of non-metallic element produces gas at cathodic discharge.Adopt the high purity graphite anode, under comparatively high temps, the chlorion discharge in the fused salt generates spontaneous the carrying out of reaction of chlorine, and the trend of impelling like this reaction (5) to carry out is larger.
In electrolytic process, adopt rare gas element to protect; Water cooling; Select quartz, glass or stainless steel as the inner casing starting material of electrolyzer, require simultaneously electrolyzer to have preferably sealing property.
Adopt the preelectrolysis process: the employing graphite carbon rod is anode, and Fe-Cr-Al wire is negative electrode.In the electrolytic furnace temperature-rise period, anode and cathode suspension are carried out preheating above fused salt.When temperature of molten salt rises to certain temperature, graphite anode and negative electrode are inserted in the fused salt, pass into direct current, under certain voltage, carry out preelectrolysis 1h, reduce impurity in the fused salt with this.
After preelectrolysis finishes; graphite anode and ready cathode steel sample are inserted in the fused salt; pass into direct current and carry out electrolysis; in whole process; all in reactor, pass into high-purity argon gas, at high temperature not oxidized with this guard reactor, and in time will react the waste gas that produces and take out of; promote the electrolysis desulphurization reaction, and the work-ing life of extension reactor.
After electrolysis finished, powered-down mentioned negative electrode to the fused salt top, during to continue to pass into high-purity argon gas and recirculated cooling water, but need argon flow amount is decreased to 1/2.When temperature of reactor drops to 500 ℃, close argon gas; When temperature of reactor is down to room temperature, close recirculated cooling water.
Embodiment
Embodiment 1
It is high that the 500g steel is made an about 5mm, and diameter is the right cylinder of 40mm, after the section fan-shaped flake is polished, is polished, until surperficial no marking.Use successively respectively clear water and alcohol wash specimen surface again, then dry up with blower, sealing is preserved.Weigh in the balance and get the certain mass muriate, it is levigate, in retort furnace, dry, for subsequent use.Before carrying out electrolysis, the resistance to air loss of inspection apparatus, the obnoxious flavour that prevents from producing in the reaction process is without filtering discharge.Heat up, the muriate that drying is good is placed in the alumina crucible, places reactor bottom, opens recirculated cooling water, and resistance furnace is warming up to 850 ℃, and heat-up rate is set to 3h, is warming up to 850 ℃ by room temperature, and soaking time is determined by experiment.Preelectrolysis: owing to may contain a certain amount of impurity in the fused salt, bring disadvantageous effect for avoiding it, need before experiment is carried out, to carry out preelectrolysis.In the preelectrolysis process, the employing graphite carbon rod is anode, and Fe-Cr-Al wire is negative electrode.In the electrolytic furnace temperature-rise period, anode and cathode suspension are carried out preheating above fused salt.When temperature of molten salt rises to 850 ℃, graphite anode and negative electrode are inserted in the fused salt, pass into direct current, under 2V voltage, carry out preelectrolysis 1h, reduce impurity in the fused salt with this.After preelectrolysis finishes; graphite anode and ready cathode steel sample are inserted in the fused salt; pass into direct current and carry out electrolysis; in whole experimentation; all in reactor, pass into high-purity argon gas, at high temperature not oxidized with this guard reactor, and in time will react the waste gas that produces and take out of; promote the electrolysis desulphurization reaction, and the work-ing life of extension reactor.After electrolysis 60 minutes, electrolysis finished, powered-down mentioned negative electrode to the fused salt top, during to continue to pass into high-purity argon gas and recirculated cooling water, but need argon flow amount is decreased to 1/2.When temperature of reactor drops to 500 ℃, close argon gas; When temperature of reactor is down to room temperature, close recirculated cooling water.
The final sulphur content of this ferrous materials is 0.0022% (massfraction), can satisfy the special steel application requiring, and the molten salt electrochemistry reduction method has the effect of the sulfide inclusion on significant removal solid steel surface.
Embodiment 2
It is high that the 500g steel is made an about 5mm, and diameter is the right cylinder of 40mm, after the section fan-shaped flake is polished, is polished, until surperficial no marking.Use successively respectively clear water and alcohol wash specimen surface again, then dry up with blower, sealing is preserved.Weigh in the balance and get the certain mass muriate, it is levigate, in retort furnace, dry, for subsequent use.Before carrying out electrolysis, the resistance to air loss of inspection apparatus, the obnoxious flavour that prevents from producing in the reaction process is without filtering discharge.Heat up, the muriate that drying is good is placed in the alumina crucible, places reactor bottom, opens recirculated cooling water, and resistance furnace is warming up to 830 ℃, and heat-up rate is set to 3h, is warming up to 830 ℃ by room temperature, and soaking time is determined by experiment.Preelectrolysis: owing to may contain a certain amount of impurity in the fused salt, bring disadvantageous effect for avoiding it, need before experiment is carried out, to carry out preelectrolysis.In the preelectrolysis process, the employing graphite carbon rod is anode, and Fe-Cr-Al wire is negative electrode.In the electrolytic furnace temperature-rise period, anode and cathode suspension are carried out preheating above fused salt.When temperature of molten salt rises to 850 ℃, graphite anode and negative electrode are inserted in the fused salt, pass into direct current, under 3V voltage, carry out preelectrolysis 1h, reduce impurity in the fused salt with this.After preelectrolysis finishes; graphite anode and ready cathode steel sample are inserted in the fused salt; pass into direct current and carry out electrolysis; in whole experimentation; all in reactor, pass into high-purity argon gas, at high temperature not oxidized with this guard reactor, and in time will react the waste gas that produces and take out of; promote the electrolysis desulphurization reaction, and the work-ing life of extension reactor.After electrolysis 100 minutes, electrolysis finished, powered-down mentioned negative electrode to the fused salt top, during to continue to pass into high-purity argon gas and recirculated cooling water, but need argon flow amount is decreased to 1/2.When temperature of reactor drops to 500 ℃, close argon gas; When temperature of reactor is down to room temperature, close recirculated cooling water.
The final sulphur content of this ferrous materials is 0.0019% (massfraction), can satisfy the special steel application requiring, and the molten salt electrochemistry reduction method has the effect of the sulfide inclusion on significant removal solid steel surface.
Claims (7)
1. the present invention utilizes the molten salt electrochemistry reduction process to remove the method for the sulfide inclusion on solid steel surface, it is characterized in that selecting muriate as molten salt electrolyte, the temperature of fused salt electrolysis is 800 ℃～900 ℃, and electrolysis voltage is 2.0～4.0V, and electrolysis time is 1 hour～3 hours.The method of the sulfide inclusion on this removal solid steel surface may further comprise the steps: fused salt is chosen and pre-treatment; Preelectrolysis and electrolytic process.
2. the method for utilizing the molten salt electrochemistry reduction process to remove the sulfide inclusion on solid steel surface as claimed in claim 1, it is characterized in that used fused salt is the muriate of alkali and alkaline earth metal ions, selection principle is: have the characteristic of non-toxic inexpensive, more stable chemical property, higher vapour pressure, less viscosity, higher conductance, with large by the density difference of Electrowinning metal, more greatly, easily electrolysate is in time separated to the interfacial tension of metal, the ability that has simultaneously stronger dissolved substance is beneficial to electrolytic process and carries out.
3. the method for utilizing the molten salt electrochemistry reduction process to remove the sulfide inclusion on solid steel surface as claimed in claim 1 is characterized in that used negative electrode is that sulfur-bearing is mingled with solid steel, and anode is high purity graphite.In the electrolytic process react into:
Cathodic reaction:
FeS+2e→Fe+S
2- (1)
S+2e→S
2- (2)
Anodic reaction:
(S
2-)
Sulfide→ (S
2-)
In the fused salt(3)
CaCl
2-2e→Ca
2++Cl
2↑ (4)
Total reaction:
CaCl
2+FeS→CaS+Fe+Cl
2↑ (5)
The step of the thionic in the steel sample is removed in reaction (1) and reaction (2).Reaction (3) is diffused in the fused salt sulfonium ion in the cathode steel sample.Reaction (4) is that the ion of non-metallic element produces gas at cathodic discharge.Adopt the high purity graphite anode, under comparatively high temps, the chlorion discharge in the fused salt generates spontaneous the carrying out of reaction of chlorine, and the trend of impelling like this reaction (5) to carry out is larger.
4. the method for utilizing the molten salt electrochemistry reduction process to remove the sulfide inclusion on solid steel surface as claimed in claim 1 is characterized in that adopting in electrolytic process rare gas element to protect; Water cooling; Select quartz, glass or stainless steel as the inner casing starting material of electrolyzer, require simultaneously electrolyzer to have preferably sealing property.
5. the method for utilizing the molten salt electrochemistry reduction process to remove the sulfide inclusion on solid steel surface as claimed in claim 1, it is characterized in that adopting the preelectrolysis process: the employing graphite carbon rod is anode, Fe-Cr-Al wire is negative electrode.In the electrolytic furnace temperature-rise period, anode and cathode suspension are carried out preheating above fused salt.When temperature of molten salt rises to certain temperature, graphite anode and negative electrode are inserted in the fused salt, pass into direct current, under certain voltage, carry out preelectrolysis 1h, reduce impurity in the fused salt with this.
6. the method for utilizing the molten salt electrochemistry reduction process to remove the sulfide inclusion on solid steel surface as claimed in claim 1; after it is characterized in that preelectrolysis finishes; graphite anode and ready cathode steel sample are inserted in the fused salt; pass into direct current and carry out electrolysis, in whole process, all will in reactor, pass into high-purity argon gas; at high temperature not oxidized with this guard reactor; and in time will react the waste gas that produces and take out of, promote the electrolysis desulphurization reaction, and the work-ing life of extension reactor.
7. the method for utilizing the molten salt electrochemistry reduction process to remove the sulfide inclusion on solid steel surface as claimed in claim 1, after it is characterized in that electrolysis finishes, powered-down, negative electrode is mentioned to the fused salt top, to continue during this time to pass into high-purity argon gas and recirculated cooling water, but need argon flow amount is decreased to 1/2.When temperature of reactor drops to 500 ℃, close argon gas; When temperature of reactor is down to room temperature, close recirculated cooling water.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108101005A (en) * | 2018-01-19 | 2018-06-01 | 广东省稀有金属研究所 | A kind of preparation method of alkaline earth sulfide |
| CN108118364A (en) * | 2018-01-19 | 2018-06-05 | 广东省稀有金属研究所 | A kind of method that metal and magnesium sulfide are prepared by metal sulfide |
| CN108360025A (en) * | 2018-05-02 | 2018-08-03 | 东北大学 | A kind of method that aqueous solution electrolysis solid metallic sulfide prepares metal |
| CN109280941A (en) * | 2018-11-16 | 2019-01-29 | 北京科技大学 | A kind of method of ferrotianium grandidierite carbon vulcanization-electrolytic preparation Titanium |
| CN110565120A (en) * | 2019-10-18 | 2019-12-13 | 东北大学 | Method for removing and recovering copper from copper-containing iron liquid |
| CN111778524A (en) * | 2020-07-28 | 2020-10-16 | 吴高武 | Leak-proof rare earth metal electrolytic tank device |
| CN112548253A (en) * | 2020-11-30 | 2021-03-26 | 哈尔滨工业大学 | Method for brazing fiber reinforced composite material and metal in selective hot corrosion auxiliary mode |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108101005A (en) * | 2018-01-19 | 2018-06-01 | 广东省稀有金属研究所 | A kind of preparation method of alkaline earth sulfide |
| CN108118364A (en) * | 2018-01-19 | 2018-06-05 | 广东省稀有金属研究所 | A kind of method that metal and magnesium sulfide are prepared by metal sulfide |
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| CN108360025A (en) * | 2018-05-02 | 2018-08-03 | 东北大学 | A kind of method that aqueous solution electrolysis solid metallic sulfide prepares metal |
| CN108360025B (en) * | 2018-05-02 | 2019-05-07 | 东北大学 | A kind of method that aqueous solution electrolysis solid metallic sulfide prepares metal |
| CN109280941A (en) * | 2018-11-16 | 2019-01-29 | 北京科技大学 | A kind of method of ferrotianium grandidierite carbon vulcanization-electrolytic preparation Titanium |
| CN109280941B (en) * | 2018-11-16 | 2020-02-28 | 北京科技大学 | Method for preparing metallic titanium by titanic iron composite ore, carbon sulfurization and electrolysis |
| CN110565120A (en) * | 2019-10-18 | 2019-12-13 | 东北大学 | Method for removing and recovering copper from copper-containing iron liquid |
| CN110565120B (en) * | 2019-10-18 | 2021-09-07 | 东北大学 | Method for removing and recovering copper from copper-containing iron liquid |
| CN111778524A (en) * | 2020-07-28 | 2020-10-16 | 吴高武 | Leak-proof rare earth metal electrolytic tank device |
| CN112548253A (en) * | 2020-11-30 | 2021-03-26 | 哈尔滨工业大学 | Method for brazing fiber reinforced composite material and metal in selective hot corrosion auxiliary mode |
| CN112548253B (en) * | 2020-11-30 | 2022-03-25 | 哈尔滨工业大学 | Method for brazing fiber reinforced composite material and metal in selective hot corrosion auxiliary mode |
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Application publication date: 20130327 |